WO2024062805A1 - Agent de prise rapide liquide et béton projeté - Google Patents

Agent de prise rapide liquide et béton projeté Download PDF

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Publication number
WO2024062805A1
WO2024062805A1 PCT/JP2023/029545 JP2023029545W WO2024062805A1 WO 2024062805 A1 WO2024062805 A1 WO 2024062805A1 JP 2023029545 W JP2023029545 W JP 2023029545W WO 2024062805 A1 WO2024062805 A1 WO 2024062805A1
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WO
WIPO (PCT)
Prior art keywords
setting agent
liquid quick
quick
ppm
less
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Application number
PCT/JP2023/029545
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English (en)
Japanese (ja)
Inventor
博貴 水野
貴光 室川
昌浩 岩崎
Original Assignee
デンカ株式会社
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Application filed by デンカ株式会社 filed Critical デンカ株式会社
Publication of WO2024062805A1 publication Critical patent/WO2024062805A1/fr

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B22/00—Use of inorganic materials as active ingredients for mortars, concrete or artificial stone, e.g. accelerators, shrinkage compensating agents
    • C04B22/06—Oxides, Hydroxides
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B22/00—Use of inorganic materials as active ingredients for mortars, concrete or artificial stone, e.g. accelerators, shrinkage compensating agents
    • C04B22/08—Acids or salts thereof
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B22/00—Use of inorganic materials as active ingredients for mortars, concrete or artificial stone, e.g. accelerators, shrinkage compensating agents
    • C04B22/08—Acids or salts thereof
    • C04B22/14—Acids or salts thereof containing sulfur in the anion, e.g. sulfides
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
    • C04B28/02—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing hydraulic cements other than calcium sulfates

Definitions

  • the present invention relates to a liquid quick-setting agent and shotcrete containing the liquid quick-setting agent.
  • a quick-setting concrete spraying method in which a quick-setting agent is mixed with concrete has been used.
  • This method involves measuring and mixing the materials in a metering plant installed at the excavation site to prepare shotcrete, pumping it, mixing it with a quick-setting agent pumped from the other side of the converging pipe, and applying it to the ground surface. This is a method of spraying until a predetermined thickness is reached.
  • the quick-setting agents used in the spraying method can be broadly classified into two types: powder quick-setting agents whose main components are calcium aluminate or alkali metal aluminate, and liquid quick-setting agents whose main components are alkali metal aluminate or aluminum sulfate.
  • liquid quick-setting admixtures have the problem of having lower quick-setting properties compared to powder quick-setting admixtures. Therefore, as a measure to improve quick-setting properties, measures have been taken to improve strength by increasing the sulfate ion concentration, as shown in Patent Document 1, for example.
  • measures have been taken to improve strength by increasing the sulfate ion concentration, as shown in Patent Document 1, for example.
  • high-concentration liquid quick-setting admixtures are stored for long periods of time, there are cases in which precipitates form in the liquid, the liquid gels, or suspended particles settle.
  • solubility of aluminum sulfate in water is 27% at 20°C, and varies depending on the coexisting solutes and the liquid temperature, but liquid quick-setting admixtures that contain aluminum sulfate above the solubility have the problem of having poor storage stability and making it difficult to maintain the properties they had immediately after production.
  • a liquid quick-setting agent made of aluminum fluoride, an acidic or basic solution of aluminum containing hydrofluoric acid of aluminum, lithium silicate, or lithium aluminate, as disclosed in Patent Document 2 is used. Proposed.
  • a liquid quick-setting agent consisting of a fluoride-containing water-soluble aluminum salt obtained by the reaction of aluminum sulfate and hydrofluoric acid, aluminum hydroxide, and lithium hydroxide, lithium carbonate, lithium sulfate, etc., as disclosed in Patent Document 3 can be used. We are doing development.
  • the present invention aims to provide a liquid quick-setting agent that has excellent quick-setting properties and storage stability, and does not contain a fluorine component, so there is no concern about fluorine elution.
  • the present inventors conducted intensive studies based on the above-mentioned problems, and as a result, the present inventors found that a material that contains an aluminum component and a sulfur component, substantially does not contain a fluorine component, and has a spectrum obtained by 27 Al-NMR.
  • the inventors have discovered that a liquid quick-setting agent having a peak at a specific chemical shift can solve the above problems, and have completed the present invention. That is, the present invention is as follows.
  • External standard Aluminum chloride aqueous solution
  • liquid quick-setting agent that has excellent quick-setting properties and storage stability, and does not contain a fluorine component, so there is no concern about fluorine elution.
  • the liquid quick-setting agent according to the present embodiment is a liquid quick-setting agent that contains an aluminum component and a sulfur component and does not substantially contain a fluorine component, and is obtained by 27 Al-NMR measured under the following conditions. It is a liquid quick-setting agent that has a peak in the chemical shift range of more than -5.0 ppm and less than 0 ppm in the spectrum. (conditions) Observation core: 27 Al Sample tube rotation speed: 12Hz Measurement temperature: 25°C Pulse width: 5 ⁇ sec (45° pulse) Waiting time: 5 seconds External standard: Aluminum chloride aqueous solution
  • the liquid quick setting agent does not substantially contain a fluorine component.
  • the fluoride ion concentration in the liquid quick setting agent is preferably less than 1.0 ppm. Although the lower limit is not limited, it may be 0 ppm.
  • the liquid quick-setting agent does not substantially contain a fluorine component, it can be a liquid quick-setting agent that has no concern about fluorine elution.
  • the fluoride ion concentration in the liquid quick-setting agent can be measured by a commercially available analyzer, for example, ion chromatography (ICS2100) manufactured by Thermo Scientific. At the time of analysis, measurement can be performed by diluting the fluoride ion in advance so that it falls within the calibration curve.
  • ICS2100 ion chromatography
  • the liquid quick setting agent has a chemical shift peak in the range of more than -5.0 ppm and less than 0 ppm, preferably in the range of -4.5 ppm or more and -1.0 ppm or less. Has a peak. If the liquid quick-setting agent does not have a peak in the chemical shift range of more than -5.0 ppm and less than 0 ppm in the spectrum obtained by 27 Al-NMR, there is a possibility that the liquid quick-setting agent does not exhibit quick setting properties.
  • the chemical shift in the spectrum obtained by 27 Al-NMR of the liquid quick-setting agent is preferably 10.0 ppm or less, and more preferably 7.0 ppm or less, in the range of more than -5.0 ppm and less than 0 ppm. , more preferably 5.0 ppm or less.
  • the half width may be, for example, 0.1 ppm or more.
  • the 27 Al-NMR measurement of the liquid quick setting agent can be performed using a commercially available measuring device, for example, a superconducting nuclear magnetic resonance apparatus (ECX-400) manufactured by JEOL Ltd., under the following conditions.
  • Observation core 27 Al Sample tube rotation speed: 12Hz
  • Measurement temperature 25°C
  • Pulse width 5 ⁇ sec (45° pulse)
  • Waiting time 5 seconds
  • External standard Aluminum chloride aqueous solution
  • the total alkali amount R 2 O (R is an alkali metal) in the liquid quick-setting admixture is preferably 1.0 mass% or less, more preferably 0.8 mass% or less, and even more preferably 0.5 mass% or less, from the viewpoint of worker safety. It may also be 0 mass% or more.
  • the total alkali amount R 2 O in the liquid quick-setting admixture can be set within the above range.
  • the total alkali amount R 2 O in the liquid quick-setting admixture can be measured by atomic absorption spectrometry.
  • the chloride ion concentration in the liquid quick-setting agent is preferably 5.0% by mass or less, more preferably 3.0% by mass or less, and even more preferably 2.0% by mass or less, from the viewpoint of preventing steel material corrosion.
  • the chloride ion concentration in the liquid quick-setting agent can be kept within the above range, for example, by using raw materials with a low chloride ion concentration.
  • the chloride ion concentration in the liquid quick-setting agent can be measured by a commercially available analyzer, for example, ion chromatography (ICS2100) manufactured by Thermo Scientific. During analysis, measurement can be performed by diluting the sample in advance so that chloride ions fall within the calibration curve.
  • ICS2100 ion chromatography
  • the liquid quick-setting agent can be obtained, for example, by mixing a raw material for an aluminum component such as aluminum sulfate, various alums, or aluminum hydroxide with a raw material for a sulfur component such as sulfuric acid, and reacting the mixture at high heat.
  • the heating temperature is preferably 70 to 100°C, more preferably 85 to 100°C, even more preferably 85 to 95°C.
  • the reaction time is preferably 30 to 150 minutes, more preferably 60 to 150 minutes, even more preferably 90 to 120 minutes. That is, for example, it can be prepared by mixing aluminum hydroxide and sulfuric acid and heating the mixture at 85 to 95° C. for 90 to 120 minutes.
  • the liquid quick-setting agent preferably contains an aluminum component of 7.2 to 20.0% by mass, more preferably 7.5 to 18.0% by mass, calculated as Al 2 O 3 , and more preferably 8.0% by mass. It is more preferable to contain up to 15.0% by mass.
  • the aluminum component in this embodiment includes aluminum atoms, and refers to, for example, aluminum ions derived from raw materials and aluminum compounds such as aluminum hydroxide. By adjusting the amount of raw material for the aluminum component used when preparing the liquid quick-setting agent, the aluminum component in the liquid quick-setting agent can be within the above range in terms of Al 2 O 3 , and the liquid quick-setting agent can be Can improve cohesion.
  • the liquid quick-setting agent preferably contains a sulfur component of 17.0 to 30.0% by mass, more preferably 19.0 to 28.0% by mass, and more preferably 20.0 to 26% by mass in terms of SO3 . It is more preferable to contain .0% by mass.
  • the sulfur component in this embodiment includes a sulfur atom, and includes, for example, sulfate ions derived from raw materials and sulfates such as magnesium sulfate.
  • the liquid quick setting agent preferably contains a magnesium component of 0.05 to 0.5% by mass, more preferably 0.06 to 0.4% by mass, and 0.07 to 0.5% by mass in terms of MgO. It is more preferable to contain 3% by mass.
  • the magnesium component in this embodiment includes a magnesium atom, and refers to, for example, a magnesium ion contained in a raw material or a magnesium compound such as magnesium oxide.
  • the liquid quick setting agent preferably contains ethanolamines in an amount of 0.5 to 5.0% by mass, more preferably 1.0 to 4.0% by mass, and 1.5 to 3.0% by mass. It is further preferable that the content be %. When the content of ethanolamines is within the above range, the storage stability of the liquid quick setting agent can be improved. Examples of ethanolamines include monoethanolamine, diethanolamine, and trimethanolamine, and from the viewpoint of storage stability, diethanolamine is preferred.
  • the liquid quick-setting agent can contain various additives as long as they do not impede the effects of the present invention, but from the viewpoint of ease of handling, it is preferable not to contain sodium aluminate.
  • the shotcrete according to the present embodiment preferably uses a combination of the liquid quick-setting agent of the present invention and a powder quick-setting agent containing calcium aluminate as a main component.
  • Shotcrete actually uses cement, but the cement used for shotcrete includes various types of Portland cement such as normal, early strength, super early strength, low heat, and medium heat, and these Portland cements.
  • Portland cement such as normal, early strength, super early strength, low heat, and medium heat
  • Cement ecocement
  • sprayed concrete uses aggregate, but there are no particular limitations on the aggregate, and it is preferable to use aggregate with low water absorption and high aggregate strength. There are no particular limitations on the maximum size of the aggregate, as long as it can be sprayed. River sand, mountain sand, sea sand, lime sand, and silica sand can be used as fine aggregate, and river gravel, mountain gravel, and lime gravel can be used as coarse aggregate, and crushed sand and crushed stone can also be used.
  • the powder quick-setting agent is preferably a powder quick-setting agent containing calcium aluminate as a main component.
  • a powder quick-setting agent containing calcium aluminate as a main component good rapid setting properties and strength development properties can be improved.
  • "containing calcium aluminate as a main component” means that the content (based on mass) of calcium aluminate is the highest among the quick-setting agent components in the powder quick-setting agent.
  • the content of calcium aluminate in the powder quick-setting agent is 30% by mass or more, preferably 30 to 80% by mass, more preferably 45 to 60% by mass. .
  • the content is 30% by mass or more, good coagulation properties can be easily obtained. Note that if the mass is 80% or less, good long-term strength development is likely to be obtained.
  • Calcium aluminate is a general term for compounds that have CaO and Al 2 O 3 as main components and have hydration activity.
  • Calcium aluminate is a substance in which a small amount of these are dissolved in solid solution in a substance whose main component is calcium aluminate, and calcium aluminate may be either crystalline or amorphous.
  • a crystalline substance if CaO is C, Al 2 O 3 is A, and R 2 O (Na 2 O, K 2 O, Li 2 O) is R, then C 3 A or an alkali metal is solidified on it.
  • Examples include dissolved C 14 RA 5 , CA, C 12 A 7 , C 11 A 7 ⁇ CaF 2 , C 4 A ⁇ Fe 2 O 3 , and C 3 A 3 ⁇ CaSO 4 , but they have good rapid setting properties. Therefore, amorphous calcium aluminate is preferable. Further, in the case of amorphous calcium aluminate, the vitrification rate is preferably 80% or more.
  • the CaO/Al 2 O 3 molar ratio of calcium aluminate is not particularly limited, but considering very early and long-term strength development, the molar ratio is preferably 2.0 to 3.0, and 2.1 to 2. .8 is more preferred. When the molar ratio is 2.0 or more, the very initial setting properties can be improved, and when it is 3.0 or less, good long-term strength development can be easily obtained.
  • a method for obtaining calcium aluminate includes heat treating a CaO raw material such as calcium carbonate or calcium hydroxide, and an Al 2 O 3 raw material such as bauxite using a rotary kiln, an electric furnace, or the like. Specifically, there is a method in which the raw materials are mixed at a predetermined ratio, heated and melted using an electric furnace, and then rapidly cooled by contacting with compressed air or water. By adjusting the ratio of each raw material, the CaO/Al 2 O 3 molar ratio can be adjusted, and the vitrification rate can be adjusted by changing the temperature during heating and melting and the cooling method.
  • the Blaine specific surface area of calcium aluminate is preferably 4000 to 8000 cm 2 /g, more preferably 5000 to 7000 cm 2 /g.
  • the Blaine specific surface area is measured based on the specific surface area test described in JIS R 5201:2015 "Physical test method for cement.”
  • the amount of liquid quick-setting agent added to the shotcrete is adjusted so that the aluminum component in the liquid quick-setting agent is preferably 0.1 to 10 parts by mass per 100 parts by mass of cement in the shotcrete. be able to. Further, the amount of the powder quick-setting agent added can be adjusted so that the amount of calcium aluminate in the powder quick-setting agent is preferably 1 to 15 parts by mass per 100 parts by mass of cement. The amount of liquid quick-setting agent and powder quick-setting agent added can be adjusted as described above according to the required strength of shotcrete, and the initial and long-term compressive strength of shotcrete can be improved. .
  • the mixing ratio of liquid quick-setting agent and powder quick-setting agent is such that, for example, if the ground condition is poor, adding a larger amount of powder quick-setting agent can improve the early strength of shotcrete. If the condition of the ground is stable, the amount of both quick-setting agents can be reduced.
  • ⁇ Preparation of liquid quick setting agent> Adjust and mix various raw materials so that the aluminum component, sulfur component, and fluorine component have the Al 2 O 3 equivalent, SO 3 equivalent, and fluoride ion concentration shown in Table 1, respectively, and heat at 90 ° C. for 2 hours. A liquid quick-setting agent was prepared.
  • Raw material for aluminum component Aluminum hydroxide, for industrial products
  • Raw material for sulfur component Sulfuric acid, for industrial products
  • Fluoride ion source Cryolite, for industrial products, contains 52-54% fluorine Solvent: Pure water
  • ⁇ Setation test/compressive strength test> A test sample was obtained by mixing 100 parts by mass of ordinary Portland cement (pH 14, industrial product), 10 parts by mass of the prepared liquid quick-setting agent, and 40 parts by mass of water (tap water). Using the obtained test samples, a setting test and a compressive strength test were conducted. The test was conducted in accordance with JIS R 5201:2015 "Physical Test Methods for Cement," and the start time, end time, and compressive strength at each age were measured. The results are shown in Table 1 below.
  • ⁇ Storage test> A storage test was conducted to evaluate the storage stability of the liquid quick setting agent. Decreased storage properties result in the formation of precipitates in the liquid accelerator, especially in low temperature environments.
  • the liquid quick-setting agent was allowed to stand in a 10° C. environment for one month, and the precipitate was extracted using filter paper, and the amount of precipitate per 100 g of the liquid quick-setting agent was calculated. The results are shown in Table 1 below.
  • JSCE-G561 ⁇ Compressive strength test>
  • the prepared shotcrete was sprayed onto a formwork, and the initial strength was measured by converting the pull-out strength at 3 hours and 1 day of age into compressive strength.
  • the shotcrete prepared according to JSCE-F561 was sprayed onto a formwork, and cores were taken at 28 days of age according to JIS A 1107:2012 to measure long-term strength.
  • the liquid quick-setting agent of the present invention can be suitably used for, for example, cement concrete sprayed onto tunnels such as roads, railways, and headrace channels, and on exposed ground surfaces such as slopes.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Curing Cements, Concrete, And Artificial Stone (AREA)
  • Testing Resistance To Weather, Investigating Materials By Mechanical Methods (AREA)
  • Lining And Supports For Tunnels (AREA)

Abstract

Un agent de prise rapide liquide qui contient un composant d'aluminium et un composant de soufre et qui est sensiblement exempt de composants de fluor, l'agent de prise rapide liquide ayant un pic dans la plage de déplacement chimique supérieur à -5,0 ppm et inférieur à 0 ppm dans un spectre obtenu par 27 Al-NMR mesuré dans les conditions suivantes. (Conditions) Noyau d'observation : 27Al. Vitesse de rotation du tube d'échantillon : 12 Hz. Température de mesure : 25 °C. Largeur d'impulsion : 5 μsec (impulsion de 45°). Temps d'attente : 5 secondes. Standard externe : solution aqueuse de chlorure d'aluminium.
PCT/JP2023/029545 2022-09-20 2023-08-15 Agent de prise rapide liquide et béton projeté WO2024062805A1 (fr)

Applications Claiming Priority (2)

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JP2022-148760 2022-09-20
JP2022148760 2022-09-20

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Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2018030731A (ja) * 2016-08-22 2018-03-01 デンカ株式会社 液体急結剤、吹付け材料及びそれを用いた吹付け工法
JP6675033B1 (ja) * 2019-08-02 2020-04-01 デンカ株式会社 セメント混和剤及び水硬性組成物
CN112608065A (zh) * 2019-12-13 2021-04-06 科之杰新材料集团(贵州)有限公司 一种喷射混凝土用液体无碱速凝剂及其制备方法
JP6873305B1 (ja) * 2020-11-09 2021-05-19 デンカ株式会社 急結性混和材、及び吹付け材料
CN113880485A (zh) * 2021-11-02 2022-01-04 北京建筑大学 一种无碱无氟液体速凝剂及制备和应用
JP6989719B1 (ja) * 2021-03-02 2022-01-05 デンカ株式会社 ２剤型急結剤、吹付け材料及び吹付け方法
CN114057422A (zh) * 2021-12-22 2022-02-18 云南云天化股份有限公司 一种无碱无氟无氯液态混凝土速凝剂及其制备方法
CN114409306A (zh) * 2022-01-06 2022-04-29 山西佳维新材料股份有限公司 一种无氟型高早强液体无碱速凝剂及制备方法和应用

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2018030731A (ja) * 2016-08-22 2018-03-01 デンカ株式会社 液体急結剤、吹付け材料及びそれを用いた吹付け工法
JP6675033B1 (ja) * 2019-08-02 2020-04-01 デンカ株式会社 セメント混和剤及び水硬性組成物
CN112608065A (zh) * 2019-12-13 2021-04-06 科之杰新材料集团(贵州)有限公司 一种喷射混凝土用液体无碱速凝剂及其制备方法
JP6873305B1 (ja) * 2020-11-09 2021-05-19 デンカ株式会社 急結性混和材、及び吹付け材料
JP6989719B1 (ja) * 2021-03-02 2022-01-05 デンカ株式会社 ２剤型急結剤、吹付け材料及び吹付け方法
CN113880485A (zh) * 2021-11-02 2022-01-04 北京建筑大学 一种无碱无氟液体速凝剂及制备和应用
CN114057422A (zh) * 2021-12-22 2022-02-18 云南云天化股份有限公司 一种无碱无氟无氯液态混凝土速凝剂及其制备方法
CN114409306A (zh) * 2022-01-06 2022-04-29 山西佳维新材料股份有限公司 一种无氟型高早强液体无碱速凝剂及制备方法和应用

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